Designation: D 453 – 94 (Reapproved 2000)e1

Standard Test Method for

Tar Acids in Creosote-Coal Tar Solutions1
This standard is issued under the fixed designation D 453; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

e1 NOTE—A keyword was added editorially in March 2000.

1. Scope 4. Significance and Use

1.1 This test method covers the determination of tar acids in 4.1 This test method covers the determination of tar acid
creosote and creosote-coal tar solution. content of creosote coal tar solutions so that comparison can be
1.1.1 Test Method D 38 covers the sampling of wood made with existing international standards, for example, Brit-
preservatives prior to testing. ish Standard 144.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5. Apparatus
responsibility of the user of this standard to establish appro- 5.1 Creosote Distillation Equipment, as described in Test
priate safety and health practices and determine the applica- Method D 246.
bility of regulatory limitations prior to use. 5.2 Separatory Funnels—Two Squibb-type separatory fun-
nels with stoppers, 250-mL capacity.
2. Referenced Documents 5.3 Type II Separatory Funnel—The Type II glass separa-
2.1 ASTM Standards: tory funnel shall have a total capacity of not less than 260 mL
D 38 Test Methods for Sampling Wood Preservatives Prior and not more than 650 mL, and shall conform to the require-
to Testing2 ments shown in Fig. 1 except that the bulb at the top may be
D 95 Test Method for Water in Petroleum Products and replaced by a 500-mL Squibb-type bulb. The capacity of the
Bituminous Materials by Distillation3 lower bulb from the stopcock to the first graduation mark shall
D 246 Test Method for Distillation of Creosote and be 65.0 mL, and above this mark the stem shall be graduated
Creosote-Coal Tar Solutions2 accurately to a total capacity of 100.0 mL in 0.2-mL incre-
D 836 Specification for Industrial Grade Benzene4 ments. The graduation marks shall be numbered for each 2 mL.
D 843 Specification for Nitration Grade Xylene4 5.4 Thermometer—An ASTM Low Softening Point Ther-
E 1 Specification for ASTM Thermometers5 mometer having a range from − 2 to 80°C conforming to the
2.2 British Wood Preserving Association Standard: requirements for Thermometer 15C as described in Specifica-
British Standard 144 on Wood Preservation6 tion E 1 or other thermometer of suitable range and precision.
6. Reagents
3. Summary of Test Method 6.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 Acoustic solution is separated and acidified with H2 SO4 used in all tests. Unless otherwise indicated, it is intended that
to liberate tar acids that are measured in a graduated funnel. all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
1
where such specifications are available. Other grades may be
This test method is under the jurisdiction of ASTM Committee D07 on Wood used, provided it is first ascertained that the reagent is of
and is the direct responsibility of Subcommittee D07.06 on Treatments for Wood
Products. sufficiently high purity to permit its use without lessening the
Current edition approved April 15, 1994. Published June 1994. Originally accuracy of the determination.
published as D 453 – 37. Last previous edition D 453 – 86. 6.2 Sodium Hydroxide Solution (20 %)—Mix 200 g of 50 %
2
Annual Book of ASTM Standards, Vol 04.10.
3
Annual Book of ASTM Standards, Vol 05.01.
sodium hydroxide (NaOH) solution with 300 g of water.
4
Annual Book of ASTM Standards, Vol 06.04. NOTE 1—Carbonate-free (clear) 50 % NaOH solution may be pur-
5
Annual Book of ASTM Standards, Vol 14.03.
6 chased and is convenient and safe to use.
Available from Premier House, 150 South Hampton Row, London, England,
WUC 1BSAL.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 453
FIG. 1 Type II Glass Separatory Funnel, 260-mL Minimum
Capacity
6.3 Sulfuric Acid Solution (40 %)—Mix 100 g of concen-
trated sulfuric acid (H2 SO 4, sp gr 1.84) carefully with stirring
into 150 g of water.
6.4 Benzene (C6 H 6)—Industrial grade, meeting the require-
ments of Specification D 836.
6.5 Xylene—(C6 H4 (CH3)2)—Nitration grade, meeting the
requirements of Specification D 843.
7. Preparation of Sample
7.1 Warm the sample, if necessary, to dissolve crystalline
material before taking portion for analysis. Determine water
content of the sample by Test Method D 95.
2
8. Procedure
8.1 Distill 100 g of the sample, weighed to the nearest 0.1 g,
to 355°C by the procedure described in Test Method D 246,
and collect the distillate in a Squibb-type separatory funnel.
Add 50 mL of C6 H6 to the freshly distilled fraction and extract
the resulting solution with three successive 30-mL portions of
20 % NaOH solution. After each portion of caustic solution is
placed in the funnel, shake vigorously, allow to settle com-
pletely, then draw off the lower layer into the second Squibb
separatory funnel before placing the next 30-mL portion in the
funnel containing the sample.
8.2 Wash the combined caustic layers in the second separa-
tory funnel with 50 mL of C6 ·H6. Draw off the washed caustic
layer into a 250-mL beaker and heat on a hot plate under an
efficient hood until the odor of benzene is no longer detectable.
Cool the NaOH solution in a water and ice bath. Then acidify
with 40 % H2 SO4 solution until the sodium sulfate solution is
definitely acid to litmus, taking care to keep the mixture cool at
all times.
8.3 Place 65 to 66 mL of C6 H4 (CH 3)2 in the Type II
separatory funnel. Submerge the lower portion of the funnel in
a water bath at room temperature. After 30 min record the
temperature of the bath to the nearest 0.1°C and read the
volume of solvent to the nearest 0.1 mL. Pour the sulfate
solution with the liberated tar acids through the solvent layer.
Draw off the sulfate solution at the bottom of the separatory
funnel into the original beaker, washing down the sides of the
beaker, and pour it back into the funnel. Repeat this operation
until all visible oil is transferred to the separatory funnel.
Finally, with all sulfate solution in the funnel, shake well and
allow to stand until the layers have separated and no drops of
solvent are dispersed in the sulfate solution. Then draw off the
sulfate layer slowly and completely, immerse the lower part of
the funnel in the water bath, and adjust the temperature to
within 0.5°C of the recorded temperature. After 30 min read the
volume of the solvent layer. The increase in volume of the
solvent is the tar acid content of the sample taken for
distillation.
9. Calculation and Report
9.1 Calculate the tar acids content of the original dry sample
as follows:
volume of tar acids, mL
weight of dry sample, g 3 100 (1)
9.2 Report tar acids as mL/100 g of dry sample.
10. Keywords
10.1 coal tar; creosote; solution; tar acids
 D 453

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